CE2SPE:

Separation Processes in Chemical and

Biochemical Engineering

Tutorial 2 Distillation:
Number of theoretical stages & Reflux
(Week 8)

Dr Vesna Najdanovic: [email protected]

Q&A
Topics

Distillation Liquid-liquid extraction

Particle Technology 1. Vapour-liquid equilibria 1. Liquid-liquid equilibria
1. Powder flow 2. McCabe Thiele method for 2. Single-stage
2. Particle shape and binary distillation extraction
size 3. Numerical Shortcut Method 3. Multistage cross-
3. Particle-fluid 4. Reflux ratio current extraction
systems: 5. Design of distillation
i) Sedimentation 4. Counter-current
columns extraction
ii) Centrifugation
5. Equipment for liquid-
liquid extraction
6. Aqueous biphasic
systems

3
Recap - q line, UOP and LOP lines
Moles of saturated liquid in the feed
q=
Total moles of feed
q 1
y= x− xF
q −1 q −1

𝑥𝐷
𝑅+1 (xF, xF)
(xF, xF)

4
 Recap - McCabe Thiele Method

1) Carry out Overall Mass Balances

2) Plot V.L.E. data and draw 45o line.
3) Plot xD, xF, xW on 45o line.
4) Plot xD/(R + 1) on Ordinate.
5) Draw ‘UOL‘ through (xD, xD) and [0, xD/(R + 1)].
6) Calculate 'q‘ and q/(q - 1).
7) Draw 'q‘ line through (xF,xF) of slope q/(q - 1).
8) Draw ‘LOL‘ from (xW,xW) to the intersection of ‘UOL‘ and the 'q'
line.
9) Step off the stages from xD to beyond xW
10) Number of Theoretical Stages = (Number of Steps - 1)

5
Recap – relative volatility
𝑦𝐴𝑥𝐵 (yA)N, (yB)N
Relative volatility 𝛼𝐴𝐵 =
𝑥𝐴𝑦𝐵
Relative volatility at the bottom: (xA)D, (xB)D

𝑦𝐴
𝑦𝐵 𝑊
𝛼𝐴𝐵 = 𝑥 (yA)D
𝑊
𝐴
𝑥𝐵 𝑊 Feed

Relative volatility at the top:

(yA)W
𝑦𝐴
𝑦𝐵 𝐷
(yA)W, (yB)W
𝛼𝐴𝐵 𝐷 = 𝑥
𝐴 (xA)W
𝑥𝐵 (xA)D
𝐷 (xA)W, (xB)W
 Recap – Fenske Equation

Average relative volatility α𝑎𝑣 = 𝛼𝐷𝛼𝑊

Fenske Equation

At total (max) reflux

 𝑳𝟎
Recap – Reflux R 𝑹=
𝑫

Optimum:
R = 1.1Rmin

8
Example 1

A distillation column is used to separate a mixture containing 63 mole % ethyl

alcohol and 37 mole % butyl acetate into a distillate of 98 mole % ethyl alcohol
and a bottom product containing 5 mole % ethyl alcohol. The feed will be liquid
at its boiling point and will enter the column at 100 kmol h-1. The column will be
operated with a reflux ratio of 1.5
• Calculate the top and bottom product flowrates.
• Estimate the number of stages.

9
 Vapour Liquid Equilibrium Data for Ethyl Alcohol – Butyl Acetate

VLE

y, Vapour phase concentration of

ethyl alcohol in mole%

x, Liquid phase concentration of

ethyl alcohol in mole%
10
Solution for Example 1

Mass balance, 1 hour

F = 100 kmol/h
XF=63% mol (ethyl alcohol)

Overall balance:
F=D+W
100 kmol = D + W D = ? kmol/h
XD=98% mol
MVC (ethyl alcohol) balance:
FxF = DxD + WxW
D
100 × 0.63 = D × 0.98 + W × 0.05
D = 62.4 kmol/h W
W = 37.6 kmol/h
W = ? kmol/h
XW =5% mol
11
Solution for Example 1 xF=63%
xD=98%
1) Carry out Overall Mass Balances xW =5%

2) Plot V.L.E. data and draw 45o line.

3) Plot xD, xF, xW on 45o line.

4) Plot xD/(R + 1) on Ordinate.

5) Draw ‘UOL‘ through (xD, xD) and

= 39.2
[0, xD/(R + 1)].

6) Calculate 'q‘ and q/(q - 1).

7) Draw 'q‘ line through (xF,xF) of

feed is liquid at its boiling
slope q/(q - 1). point q = 1
8) Draw ‘LOL‘ from (xW,xW) to the xW = 5% xF = 63% xD = 98%
intersection of ‘UOL‘ and the 'q' line.
Solution for Example 1
1
2
9) Step off the stages from xD
3
to beyond xW 4
10) Number of Theoretical

Stages = (Number of Steps - 1)

5

N=6–1 =5

xW = 5% xF = 63% xD = 98%
 Example 2
A distillation column is used to separate a mixture containing 0.20 mole fraction of A in the feed into
a top product of 0.95 mole fraction A and a bottom product containing 0.02 mole fraction A. The
feed is liquid at its boiling point. The vapour leaving the column is condensed but not cooled, and
the reflux ratio is 9:1.
1

yA
Calculate: 0.9

(a) the number of theoretical plates required 0.8

using McCabe Thiele method; 0.7

(b) compare the result in a) with the one 0.6

obtained by Fenske equation; 0.5
(c) The minimum reflux ratio for the system. 0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA 14
 Solution for Example 2 a)
(a) the number of theoretical plates required using McCabe Thiele method;
1
1) Carry out Overall Mass Balances

yA
0.9
2) Plot V.L.E. data and draw 45o line.
0.8
3) Plot xD, xF, xW on 45o line.
0.7

4) Plot xD/(R + 1) on Ordinate (=0.95/(9+1)=0.095) 0.6

5) Draw ‘UOL‘ through (xD, xD) and [0, xD/(R + 1)]. 0.5

6) Calculate 'q‘ and q/(q - 1) (q=1) 0.4

7) Draw 'q‘ line through (xF,xF) of slope q/(q - 1). 0.3

0.2
8) Draw ‘LOL‘ from (xW,xW) to the

intersection of ‘UOL‘ and the 'q' line. 0.0950.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xW = 0.02 xF = 0.2 xA
xD15= 0.95
 Solution for Example 2 a)
1
9) Step off the stages from xD

yA
0.9
to beyond xW 0.8

10) Number of Theoretical 0.7

0.6
Stages = (15 - 1) = 14
0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xW = 0.02 xF = 0.2 xA
xD = 0.95
16
 Solution for Example 2 b)
1
b) N by Fenske equation
yD = 0.96 (A)

yA
0.9
yD = 0.04 (B)
0.8

0.7
α𝑎𝑣 = 𝛼𝐷𝛼𝑊
0.6

𝑦𝐴 𝑥𝐵 0.04 ∙ 1 − 0.02 0.5

𝛼𝐴𝐵 𝑤 = = = 2.042
𝑥𝐴 𝑦𝐵 0.02 ∙ (1 − 0.04)
𝑤 0.4

𝑦𝐴 𝑥𝐵 0.96 1 − 0.95 0.3

𝛼𝐴𝐵 𝐷 = = = 1.263
𝑥𝐴 𝑦𝐵 0.95 1 − 0.96 0.2
𝐷
yW = 0.04 (A)0.1
α𝑎𝑣 = 𝛼𝐷𝛼𝑊 = 1.613 yW = 0.96 (B)
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
log (1 − 0.02)/0.02) 0.95/(1 − 0.95)
𝑁+1= xW = 0.02 (A) xA
log(1.613) Xw = 0.98 (B) xD = 0.95 (A)
xD = 0.05 (B)
𝑁 + 1 = 14.3 𝑁 = 13.3 (14 theoretical stages) 17
 Solution for Example 2 c)
c) The minimum reflux ratio for the system. 1

yA
0.9

1. q-line and xF = 0.2 0.8

2. Pinch point 0.7

3. (xD, xD) 0.6

4. Plot UOL by connecting Pinch point and (xD, xD) 0.5

xD
5. =0.15 (ordinate where UOL cuts y axis) 0.4
Rm+1
0.3
Rm = 5.3
0.2
0.15
0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xF = 0.2 xA
xD = 0.95
18
Example 3
A binary mixture of cyclohexane and toluene containing 62.2% cyclohexane is to be separated in a continuous
fractionating column. The top product is to contain 96.3% cyclohexane and the bottom product is to contain at
least 96.7% toluene.
The feed to the column is 50% liquid at its boiling point and 50% dry saturated vapour, and the vapour leaving
the column is condensed but not cooled. The equilibrium data for the mixture, in terms of the more volatile
component are in the diagram.

Calculate:

(a) the minimum reflux ratio;

(b) the number of theoretical stages required under the following reflux conditions using McCabe
Thiele method:
(i) 2:1;
(ii) 5:1;
(iii) maximum reflux.

19
Example 3 – VLE diagram
1

ycyclohexane
0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xcyclohexane

20
 Solution for Example 3 a)
(a) the minimum reflux ratio
1

yA
1. q-line and xF (q=0.5, so slope =0.5/(0.5- 0.9

0.8
1) = -1, -45o)
0.7
2. Pinch point
0.6
3. (xD, xD) xD
= 0.460.5
4. Plot UOL by connecting Pinch point Rm+1
0.4

and (xD, xD) 0.3

Minimum
xD 0.2
5. from ordinate where UOL reflux ratio
Rm+1 0.1

cuts y axis 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xD, =0.963 xA 0.622 0.963

Rm = 0.963/0.46 – 1 = 1.1
21
 Solution for Example 3 b) i)
(b) the number of theoretical stages required under the following reflux conditions using
both McCabe Thiele: (i) 2:1;
1

yA
1) Carry out Overall Mass Balances
0.9

2) Plot V.L.E. data and draw 45o line. 0.8

0.7
3) Plot xD, xF, xW on 45o line.
0.6
4) Plot xD/(R + 1) on Ordinate (=0.963/(2+1)=0.32)
0.5
5) Draw ‘UOL‘ through (xD, xD) and [0, xD/(R + 1)].
xD 0.4
= 0.32
6) Calculate 'q‘ and q/(q - 1) = -1 (-45o) Rm+1 0.3

0.2
7) Draw 'q‘ line through (xF,xF) of slope q/(q - 1).
0.1
8) Draw ‘LOL‘ from (xW,xW) to the 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
intersection of ‘UOL‘ and the 'q' line. xw = 0.033 xA xF =0.622 xD = 0.963
(1-0.967)
22
 Solution for Example 3 b) i)

9) Step off the stages from xD 1

yA
0.9
to beyond xW
0.8

10) Number of Theoretical 0.7

0.6
Stages = (12 - 1) = 11
0.5

xD 0.4
= 0.32
Rm+1 0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xw = 0.033 xA xF =0.622 xD = 0.963
(1-0.967)

23
 Final answer for Example 3 b) ii)

• Number of theoretical trays= 9

24
 Solution for Example 3 b) iii)
b) iii) the number of theoretical stages required under the following reflux conditions
using McCabe Thiele: maximum reflux
1

yA
0.9
R = maximum (total) reflux ratio
0.8
(UOL and LOL are the same line, x = y)
0.7

Step off the stages from xD to beyond xW 0.6

0.5

N = 8 – 1 = 7 theoretical stages (trays) 0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xw = 0.033 xA xF =0.622 xD = 0.963
(1-0.967)
25
Example 4

A distillation column is used to separate a saturated liquid feed of two components A and B in
which the mole fraction of A is 0.40. Samples withdrawn from three successive plates between
the feed plate and the total condenser have the following composition:

Plate Vapour Liquid

yA xA
Top (T) 0.680
T-1 0.740 0.600
T-2 0.679 0.510

It is assumed that there is constant molar overflow. Determine the reflux ratio at which the column
is operating.

26
 Plate Vapour Liquid
Solution for Example 4 yA xA
Top (T) 0.680
(The reflux ratio at which the column is operating;
T-1 0.740 0.600
T-2 0.679 0.510
yT, V condenser
Material balance around plate T-1:
xT = yT, L xD = xT = yT, D
yT-2V + xTL = yT-1V + xT-1L
Top
yT-1, V xT, L 𝐿
𝑅= Solve for L/V:
𝐷
𝐿 𝑦𝑇−1 − 𝑦𝑇−2 0.74 − 0.679
= = = 0.763
T-1 𝑉 𝑥𝑇 − 𝑥𝑇−1 0.68 − 0.6

Calculate the reflux ratio:

𝐿
yT-2, V xT-1, L 𝐿 𝐿 0.763
𝑅= = = =𝑉 = 3.22
T-2
𝐷 𝑉 − 𝐿 1 − 𝐿 1 − 0.763
𝑉
27
Diagrams

28
Example 1 Vapour Liquid Equilibrium Data for Ethyl Alcohol – Butyl Acetate

y, Vapour phase concentration of

ethyl alcohol in mole%

x, Liquid phase concentration of

ethyl alcohol in mole%
29
Example 2 1

yA
0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA
30
 1

yA
Example 3 0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA
31